# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2014

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#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
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#  fide research purposes only. It may contain copyright material
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data_cait252

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4.50 H5 B0.50 N3 Pu0.17'
_chemical_formula_weight         146.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pu Pu -9.4100 4.3056 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_H-M_alt        'P 63/m'
_space_group_name_Hall           '-P 6c'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'

_cell_length_a                   11.7036(5)
_cell_length_b                   11.7036(5)
_cell_length_c                   13.5561(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1608.07(17)
_cell_formula_units_Z            12
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9535
_cell_measurement_theta_min      2.508
_cell_measurement_theta_max      27.41

_exptl_crystal_description       prism
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_F_000             854
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.118
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.064
_exptl_absorpt_coefficient_mu    2.102
_shelx_estimated_absorpt_T_min   0.790
_shelx_estimated_absorpt_T_max   0.877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.862
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_process_details   (sadabs)

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed I\ms tube'
_diffrn_measurement_device_type  'Bruker APEX II Quazar'
_diffrn_measurement_method       'combined φ- and ω-scans'
_diffrn_detector_area_resol_mean 66
_diffrn_reflns_number            28954
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.009
_diffrn_reflns_theta_max         28.452
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1381
_reflns_number_gt                1269
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX II (Bruker, 2007)'
_computing_cell_refinement       'APEX II (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0141P)²+0.9820P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1381
_refine_ls_number_parameters     108
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0178
_refine_ls_R_factor_gt           0.0149
_refine_ls_wR_factor_ref         0.0318
_refine_ls_wR_factor_gt          0.0311
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pu1 Pu 0.3333 0.6667 0.7500 0.00921(5) Uani 1 6 d S T P . .
N1 N 0.29119(14) 0.81274(14) 0.87099(12) 0.0149(3) Uani 1 1 d . . . . .
N2 N 0.22927(14) 0.88160(14) 0.84470(12) 0.0144(3) Uani 1 1 d . . . . .
N3 N 0.0743(2) 0.6103(2) 0.7500 0.0140(4) Uani 1 2 d S T P . .
N4 N 0.0401(2) 0.7064(2) 0.7500 0.0134(4) Uani 1 2 d S T P . .
C1 C 0.34502(18) 0.85975(18) 0.95925(14) 0.0169(4) Uani 1 1 d . . . . .
C2 C 0.31928(18) 0.95743(19) 0.99130(15) 0.0200(4) Uani 1 1 d . . . . .
C3 C 0.24580(18) 0.96822(18) 0.91688(14) 0.0183(4) Uani 1 1 d . . . . .
C4 C -0.0403(3) 0.4962(3) 0.7500 0.0210(6) Uani 1 2 d S T P . .
C5 C -0.1474(3) 0.5182(3) 0.7500 0.0267(7) Uani 1 2 d S T P . .
C6 C -0.0916(3) 0.6527(3) 0.7500 0.0188(6) Uani 1 2 d S T P . .
B1 B 0.1459(3) 0.8525(3) 0.7500 0.0146(6) Uani 1 2 d S T P . .
H1 H 0.3927(18) 0.8243(19) 0.9910(16) 0.018(5) Uiso 1 1 d . . . . .
H2 H 0.345(2) 1.005(2) 1.0492(19) 0.027(7) Uiso 1 1 d . . . . .
H3 H 0.209(2) 1.025(2) 0.9117(17) 0.025(6) Uiso 1 1 d . . . . .
H4 H -0.039(3) 0.415(3) 0.7500 0.027(9) Uiso 1 2 d S . P . .
H5 H -0.238(4) 0.456(4) 0.7500 0.038(10) Uiso 1 2 d S . P . .
H6 H -0.129(3) 0.707(3) 0.7500 0.022(8) Uiso 1 2 d S . P . .
H7 H 0.100(3) 0.914(3) 0.7500 0.013(7) Uiso 1 2 d S . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pu1 N1 2.5883(15) 10_557 ?
Pu1 N1 2.5883(15) 11_667 ?
Pu1 N1 2.5883(15) 2_665 ?
Pu1 N1 2.5883(15) 3_565 ?
Pu1 N1 2.5883(15) 12_567 ?
Pu1 N1 2.5883(15) . ?
Pu1 N3 2.762(2) 3_565 ?
Pu1 N3 2.762(2) . ?
Pu1 N3 2.762(2) 2_665 ?
N1 C1 1.336(2) . ?
N1 N2 1.373(2) . ?
N2 C3 1.351(2) . ?
N2 B1 1.544(2) . ?
N3 C4 1.338(3) . ?
N3 N4 1.369(3) . ?
N4 C6 1.342(3) . ?
N4 B1 1.530(4) . ?
C1 C2 1.389(3) . ?
C2 C3 1.372(3) . ?
C4 C5 1.400(4) . ?
C5 C6 1.370(4) . ?
B1 N2 1.544(2) 10_557 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Pu1 N1 84.13(5) 10_557 11_667 ?
N1 Pu1 N1 134.49(2) 10_557 2_665 ?
N1 Pu1 N1 78.64(7) 11_667 2_665 ?
N1 Pu1 N1 134.49(2) 10_557 3_565 ?
N1 Pu1 N1 134.49(2) 11_667 3_565 ?
N1 Pu1 N1 84.13(5) 2_665 3_565 ?
N1 Pu1 N1 84.13(5) 10_557 12_567 ?
N1 Pu1 N1 84.13(5) 11_667 12_567 ?
N1 Pu1 N1 134.49(2) 2_665 12_567 ?
N1 Pu1 N1 78.64(7) 3_565 12_567 ?
N1 Pu1 N1 78.64(7) 10_557 . ?
N1 Pu1 N1 134.49(2) 11_667 . ?
N1 Pu1 N1 84.13(5) 2_665 . ?
N1 Pu1 N1 84.13(5) 3_565 . ?
N1 Pu1 N1 134.49(2) 12_567 . ?
N1 Pu1 N3 67.53(4) 10_557 3_565 ?
N1 Pu1 N3 140.68(3) 11_667 3_565 ?
N1 Pu1 N3 140.68(3) 2_665 3_565 ?
N1 Pu1 N3 66.96(4) 3_565 3_565 ?
N1 Pu1 N3 66.96(4) 12_567 3_565 ?
N1 Pu1 N3 67.52(4) . 3_565 ?
N1 Pu1 N3 66.96(4) 10_557 . ?
N1 Pu1 N3 67.53(4) 11_667 . ?
N1 Pu1 N3 67.53(4) 2_665 . ?
N1 Pu1 N3 140.68(3) 3_565 . ?
N1 Pu1 N3 140.68(3) 12_567 . ?
N1 Pu1 N3 66.96(4) . . ?
N3 Pu1 N3 120.0 3_565 . ?
N1 Pu1 N3 140.68(3) 10_557 2_665 ?
N1 Pu1 N3 66.96(4) 11_667 2_665 ?
N1 Pu1 N3 66.96(4) 2_665 2_665 ?
N1 Pu1 N3 67.53(4) 3_565 2_665 ?
N1 Pu1 N3 67.53(4) 12_567 2_665 ?
N1 Pu1 N3 140.68(3) . 2_665 ?
N3 Pu1 N3 120.000(1) 3_565 2_665 ?
N3 Pu1 N3 120.001(1) . 2_665 ?
C1 N1 N2 105.62(15) . . ?
C1 N1 Pu1 129.29(12) . . ?
N2 N1 Pu1 123.64(11) . . ?
C3 N2 N1 109.44(15) . . ?
C3 N2 B1 127.25(17) . . ?
N1 N2 B1 123.15(16) . . ?
C4 N3 N4 105.1(2) . . ?
C4 N3 Pu1 132.14(17) . . ?
N4 N3 Pu1 122.72(15) . . ?
C6 N4 N3 110.7(2) . . ?
C6 N4 B1 128.4(2) . . ?
N3 N4 B1 120.8(2) . . ?
N1 C1 C2 111.55(17) . . ?
C3 C2 C1 104.45(17) . . ?
N2 C3 C2 108.94(17) . . ?
N3 C4 C5 111.1(2) . . ?
C6 C5 C4 104.7(2) . . ?
N4 C6 C5 108.3(2) . . ?
N4 B1 N2 108.41(14) . 10_557 ?
N4 B1 N2 108.41(14) . . ?
N2 B1 N2 112.5(2) 10_557 . ?

_refine_diff_density_max         0.593
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.081

_shelxl_version_number           2013-2

_database_code_depnum_ccdc_archive 'CCDC 994710'
